Process for reactivation of catalyst used for the hydrogenation of hydrocarbon oils



/Patented Jan. 17, 1933 UNITED STATES PATENT OFFICE nnwarm B. rnox, orELIZABETH, NEW JERSEY, assrenon 'ro STANDARD-I. G.

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PROCESS FOR BEACTIVATION OF CATALYST USED FOR THE HYDROGENATION OFHYDBOCABBON OILS No Drawing.

can be readily reactivated by treatment withv hydrogen either atordinary temperatures or elevated temperatures and at either low or highpressure. I 1

Catalytic destructive hydrogenation may 2 he carried out in any wellknown manner, for

catalyst may be held at an elevated temperature, say above about 7 50 F.and under hydrogen pressure in excess of about 50 atmospheres. Hydrogenor gas containing substantial quantities of free hydrogen is forced intothe oil continuously and either oil vapor alone or both liquid and vaporare removed. Fresh oil may also be added.

The catalyst may beremoved continuously or at intervals and separatedfrom the bulk of the oil by centrifugal action, settling or filtrationor any. other suitable mechanical means and then the catalyst issubjected to the action of a stream of gas comprising hydrogen ofsubstantial purity. During such treatment temperature may be normal orhigher but preferably below about 700 F. Pressure may be at atmosphericbut it is advantageous for it to be higher, say above 50 atmospheres.

dition of the spent catalyst and the nature of 3 its composition but ingeneral treatment should be from 2 to 12 hours or more. The

catalyst is then suspended in oil, for example,

the fresh feed and returned to the retort to further use.

I have found that the gas from the hydro genation retort containingprincipally -hydrogen with, hydrocarbons and hydrogen sulexample, a bodyof oil containing suspended The time of treatment difi'ers with the con-Application filed November 13, 1929. Serial No. 407,019.

phide in less proportion is a suitable reactivating medium but it ispreferable to scrub this gas with oil under pressure to remove the majorquantity of hydrocarbon constituents prior to its use, If an unscrubbedgas is used, I find it desirable to pass hydrogen of substantial purityover the catalyst for a short time before returning it to thehydrogenation retort. lDiluents such as C0, C0 and N are notobjectionable, but the amount of hydrocarbons should be kept low in thereactivating gas.

The catalysts referred to above comprise the oxides or sulphides ofchromium, molybdenum, tungsten and similar high atomic Weight elementseither alone or in admixture with each other or with the oxides orsulphides of such metals as those of the alkali, alkaline earth and rareearth groups, aluminum, zinc and the-like. All of these materials aresulphacfifte, that is are immune to poisoning by sulfur.

My invention is not to be limited by any theory of the mechanism of thereactivation process, nor to any details which may have been includedfor illustrative purposes, but only by the following claims in which Iwish to claim all novelty inherent in my invention.

claim:

1. An improved process for reactivating sulphactive catalyst used fordestructive hydrogenation of hydrocarbon oil, which'eomprises separatinthe bulk of the oil from the catalyst and sub ecting the catalyst for aprolonged period to the action of a gas comprising free hydrogensubstantially free of hydrocarbons.

2. improved process according to claim It, in which the reactivation isaccomplished 9 at an elevated temperature. i

3. An improved process according to claim 1, in which the reactivationisaccomplished under pressure in excess of 50 atmospheres.

4:. An improved process for the reactivaincomes vapors derived from thehydrogenation retort,

5. Process according cisi zl 4: in which the vapors from thehydrogenation retort are scrubbed with oil under pressure to remove themajor quantity or" iiq iiid hydrocarbon prior to passage through thespent catalyst, 6. Process according to claim 4-, which hydrogensubstantially free of hydrocarbon 1 is passed through'the catalyst for ashort period after passage of vapor derived from the h drogenationretort" 7. in improved process for the resctivw tion of spentsuiphactive catalyst used for the destructive hydrogenation ofhydrocarbon oils, which comprises removing the built of the oil andsubjecting the spent solid; catalyst to the action of gas containing asubstantial proportion of free hydrogen'at temperature below about 700Ft 8. An improved process for the reactivetion of spentisulphactivecatalyst used for the destructive hydrogenation of hydrocarbon oils,which comprises removing bulk of the oil and subjecting the spent soiidcats-' iyst to the action of gas containi e; substantial proportion offree hydrogen at tempers ture below about 709 F under pressure or inexcess of 56 atmospheres 4 39

